Department of Chemistry, Yeungnam University, Gyeongsan 712-749, South Korea.
J Chromatogr A. 2010 Jun 25;1217(26):4494-500. doi: 10.1016/j.chroma.2010.04.044. Epub 2010 Apr 22.
This work reports the preparation of monolithic zirconia chiral columns for separation of enantiomeric compounds by capillary electrochromatography (CEC). Using sol-gel technology, a porous monolith having interconnected globular-like structure with through-pores is synthesized in the capillary column as a first step in the synthesis of monolithic zirconia chiral capillary columns. In the second step, the surface of the monolith is modified by coating with cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) as the chiral stationary phase to obtain a chiral column (CDMPCZM). The process of the preparation of the zirconia monolithic capillary column was investigated by varying the concentrations of the components of the sol solution including polyethylene glycol, water and acetic acid. CDMPCZM is mechanically stable and no bubble formation was detected with the applied current of up to 30 microA. The enantioseparation behavior of the CDMPCZM columns was investigated by separating a set of 10 representative chiral compounds by varying the applied voltage and pH and organic composition of the aqueous organic mobile phases.
本工作报道了通过胶束电动色谱(CEC)制备用于拆分对映体化合物的整体氧化锆手性柱。首先采用溶胶-凝胶技术在毛细管柱中合成具有相互连通的球形结构和贯穿孔的多孔整体,作为制备整体氧化锆手性毛细管柱的第一步。在第二步中,通过涂覆纤维素三(3,5-二甲基苯基氨基甲酸酯)(CDMPC)作为手性固定相对整体进行修饰,得到手性柱(CDMPCZM)。通过改变溶胶溶液中包括聚乙二醇、水和乙酸的成分的浓度来研究氧化锆整体毛细管柱的制备过程。CDMPCZM 机械稳定,在高达 30 μA 的施加电流下未检测到气泡形成。通过改变施加电压和 pH 值以及水相有机流动相的有机组成来分离一组 10 种代表性的手性化合物,研究了 CDMPCZM 柱的对映体分离行为。